CN102918112B - For smelting process resin blend, resin particle, use them to prepare method and the resin of resin - Google Patents
For smelting process resin blend, resin particle, use them to prepare method and the resin of resin Download PDFInfo
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- CN102918112B CN102918112B CN201180026466.3A CN201180026466A CN102918112B CN 102918112 B CN102918112 B CN 102918112B CN 201180026466 A CN201180026466 A CN 201180026466A CN 102918112 B CN102918112 B CN 102918112B
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- resin
- fluorine
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- blend
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- 229920005989 resin Polymers 0.000 title claims abstract description 603
- 239000011347 resin Substances 0.000 title claims abstract description 603
- 239000000203 mixture Substances 0.000 title claims abstract description 118
- 238000000034 method Methods 0.000 title claims abstract description 101
- 230000008569 process Effects 0.000 title claims abstract description 39
- 238000003723 Smelting Methods 0.000 title claims abstract description 28
- 239000002245 particle Substances 0.000 title claims description 29
- 239000011737 fluorine Substances 0.000 claims abstract description 56
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 56
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 51
- 238000009826 distribution Methods 0.000 claims description 21
- 238000012545 processing Methods 0.000 claims description 14
- 239000000155 melt Substances 0.000 claims description 12
- 229910052799 carbon Inorganic materials 0.000 claims description 11
- AHHWIHXENZJRFG-UHFFFAOYSA-N oxetane Chemical compound C1COC1 AHHWIHXENZJRFG-UHFFFAOYSA-N 0.000 claims description 10
- 150000002148 esters Chemical class 0.000 claims description 9
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 7
- 238000006116 polymerization reaction Methods 0.000 claims description 7
- 238000010008 shearing Methods 0.000 claims description 7
- 239000004925 Acrylic resin Substances 0.000 claims description 6
- 229920000178 Acrylic resin Polymers 0.000 claims description 6
- 238000002844 melting Methods 0.000 claims description 6
- 230000008018 melting Effects 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 4
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- 125000000217 alkyl group Chemical group 0.000 description 2
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 description 2
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- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
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- KJRCEJOSASVSRA-UHFFFAOYSA-N propane-2-thiol Chemical group CC(C)S KJRCEJOSASVSRA-UHFFFAOYSA-N 0.000 description 2
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- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 2
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- OUPZKGBUJRBPGC-UHFFFAOYSA-N 1,3,5-tris(oxiran-2-ylmethyl)-1,3,5-triazinane-2,4,6-trione Chemical compound O=C1N(CC2OC2)C(=O)N(CC2OC2)C(=O)N1CC1CO1 OUPZKGBUJRBPGC-UHFFFAOYSA-N 0.000 description 1
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- FZYCEURIEDTWNS-UHFFFAOYSA-N prop-1-en-2-ylbenzene Chemical compound CC(=C)C1=CC=CC=C1.CC(=C)C1=CC=CC=C1 FZYCEURIEDTWNS-UHFFFAOYSA-N 0.000 description 1
- VVWRJUBEIPHGQF-UHFFFAOYSA-N propan-2-yl n-propan-2-yloxycarbonyliminocarbamate Chemical compound CC(C)OC(=O)N=NC(=O)OC(C)C VVWRJUBEIPHGQF-UHFFFAOYSA-N 0.000 description 1
- NHARPDSAXCBDDR-UHFFFAOYSA-N propyl 2-methylprop-2-enoate Chemical compound CCCOC(=O)C(C)=C NHARPDSAXCBDDR-UHFFFAOYSA-N 0.000 description 1
- PNXMTCDJUBJHQJ-UHFFFAOYSA-N propyl prop-2-enoate Chemical compound CCCOC(=O)C=C PNXMTCDJUBJHQJ-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 229920006132 styrene block copolymer Polymers 0.000 description 1
- 238000005211 surface analysis Methods 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
- 229920002397 thermoplastic olefin Polymers 0.000 description 1
- 231100000167 toxic agent Toxicity 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 description 1
- LPUCKLOWOWADAC-UHFFFAOYSA-M tributylstannyl 2-methylprop-2-enoate Chemical compound CCCC[Sn](CCCC)(CCCC)OC(=O)C(C)=C LPUCKLOWOWADAC-UHFFFAOYSA-M 0.000 description 1
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 1
- 229940078499 tricalcium phosphate Drugs 0.000 description 1
- 229910000391 tricalcium phosphate Inorganic materials 0.000 description 1
- 235000019731 tricalcium phosphate Nutrition 0.000 description 1
- 125000004205 trifluoroethyl group Chemical group [H]C([H])(*)C(F)(F)F 0.000 description 1
- 125000002023 trifluoromethyl group Chemical group FC(F)(F)* 0.000 description 1
- 125000000725 trifluoropropyl group Chemical group [H]C([H])(*)C([H])([H])C(F)(F)F 0.000 description 1
Classifications
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- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/12—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
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- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
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- B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
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- B32B7/02—Physical, chemical or physicochemical properties
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- C08L33/04—Homopolymers or copolymers of esters
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C08L33/04—Homopolymers or copolymers of esters
- C08L33/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, which oxygen atoms are present only as part of the carboxyl radical
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- B32B2437/00—Clothing
- B32B2437/04—Caps, helmets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- C08J2400/10—Polymers characterised by the presence of specified groups, e.g. terminal or pendant functional groups
- C08J2400/102—Polymers characterised by the presence of specified groups, e.g. terminal or pendant functional groups containing halogen atoms
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
- Y10T428/2991—Coated
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
- Y10T428/2991—Coated
- Y10T428/2998—Coated including synthetic resin or polymer
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/31504—Composite [nonstructural laminate]
- Y10T428/3154—Of fluorinated addition polymer from unsaturated monomers
Landscapes
- Chemical & Material Sciences (AREA)
- Medicinal Chemistry (AREA)
- Organic Chemistry (AREA)
- Polymers & Plastics (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Engineering & Computer Science (AREA)
- Injection Moulding Of Plastics Or The Like (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
- Laminated Bodies (AREA)
Abstract
The invention provides a kind of resin blend for smelting process, use this resin blend to prepare method and the resin of resin.This resin blend can comprise: the first resin, and the second resin, and described second resin comprises the resin of the organo-functional group introducing fluorine or fluorine replacement, and the surface energy differential of the second resin and described first resin is 0.1 ~ 35mN/m described in 25 ° of C.Due to this resin blend, the mechanical property of resin and surface property can improve, and excellent contamination resistance can realize.In addition, do not need coating or coating owing to manufacturing resin, so manufacturing time and/or manufacturing cost can reduce, and productivity can improve.
Description
Technical field
The present invention relates to a kind of resin blend for smelting process, resin particle, them are used to prepare method and the resin of resin, more specifically, relate to a kind of resin blend for smelting process, this resin blend can improve mechanical property and the surface property of resin, realize excellent contamination resistance and improve manufacturing efficiency, such as, reduce process period, boost productivity, and do not use extra top coat and reduce manufacturing cost, the present invention relates to a kind of resin particle, them are used to prepare method and the resin of resin.
Background technology
Due to the processing characteristics of resin excellence and the performance of excellent such as tensile strength, Young's modulus, thermotolerance and shock resistance, so resin is used in multiple application, the parts of the parts of such as automobile, the helmet, electrical means, the parts of spinning-drawing machine, toy or pipe.
Particularly, because and direct body contact, so require that the resin being used for household indoor decoration, trolley part and toy is eco-friendly, and there is excellent resistance to marring.But when resin is exposed to outside atmosphere for some time, this resin decomposes because of the oxygen in air, ozone and light usually, and color easily changes.Therefore, this resin becomes non-constant in weathering resistance and intensity, and is easy to broken.In addition, due to thermoplastic resin to be easy to by dust, water or oil stain, so proposed to use anti-contamination coating agent or UV coating to the method for resin coating and coating, improved the surface property of Plastic Resin.
But such coating or method of coating can reduce efficiency and the economic feasibility of resin manufacture method, or produce toxic substance in the processing or treating processes of rosin products.In addition, coatingsurface departs from, and is difficult to show physicals consistently.
Therefore, propose multiple method to improve the performance of Plastic Resin, such as resistance to marring or contamination resistance, and do not adopt the method for coating or coating.Such as, proposed inorganic particulate to join method in resin to improve the physicals of resin, such as wear resistance and hardness.But the method may the processibility of deteriorated resin and shock strength and gloss characteristic.Although also proposed the resin that adds in addition and there is excellent resistance to marring or contamination resistance to improve the method for the surface property of Plastic Resin, but according to the method, need extra technique, curing process such as after injecting products, and physicals (such as contamination resistance) may not be improved to the degree required by this product.
Due to these reasons, need a kind of when not using improving the efficiency of technique and economic feasibility when Plastic Resin coating or the technique of coating and improving the mechanical property of goods and the method for contamination resistance.
Summary of the invention
Technical problem
The invention provides a kind of such as extruding for smelting process or the resin blend (resinblend) of injection moulding (injection).Described resin blend can improve mechanical property and the surface property contamination resistance that also realization is excellent of resin.In addition, owing to not needing coating or coating for manufacture resin, so manufacturing time and/or manufacturing cost can reduce, and productivity can improve.
The present invention also provides by using the described resin particle for the resin blend of smelting process.
The present invention also provides again a kind of by using the described resin blend for smelting process to prepare the method for resin.
The present invention also provides again a kind of resin with the melt-processed of the surface property (such as contamination resistance) of improvement.
Technical scheme
In one embodiment, the resin blend for smelting process comprises: the first resin; Second resin, described second resin comprises the resin of the organo-functional group introducing fluorine or fluorine replacement, and the surface energy differential of described second resin and described first resin is 0.1 ~ 35mN/m at 25 ° of C.
In another embodiment, resin particle comprises: the core comprising the first resin; With the shell comprising the second resin, described second resin comprises the resin of the organo-functional group introducing fluorine or fluorine replacement, and the surface energy differential of described second resin and described first resin is 0.1 ~ 35mN/m at 25 ° of C.
Going back in an embodiment, the method preparing resin comprises makes described resin blend melting to form mixture of melts and to process this mixture of melts.
In yet another embodiment, the resin of melt-processed comprises: the first resin layer; The second resin layer that described first resin layer is formed; Comprise the first resin and the second resin and the interfacial layer formed between described first resin layer and the second resin layer.Herein, described second resin layer comprises the resin of the organo-functional group introducing fluorine or fluorine replacement.
In another embodiment, the resin of melt-processed comprises: the first resin layer; With the second resin layer formed on described first resin layer.From the surface of described second resin layer, the composition of the first resin layer adopts infrared (IR) spectrograph to detect, and described second resin layer comprises the resin of the organo-functional group introducing fluorine or fluorine replacement.
Hereinafter, detailed description is used for according to embodiments of the present invention resin blend, the resin particle of smelting process, uses them to prepare method and the resin of resin.
In the present invention, blend can be a kind of blend that wherein the first resin and the second resin are evenly blended in a kind of matrix, or the resin particle be wherein made up of the first resin and the evenly blended a kind of blend of the resin particle that is made up of the second resin.The blend that wherein resin is evenly blended in a kind of matrix refers to that the first resin and the second resin are blended in a kind of resin particle equably, thus presents with a kind of form of composition.
Smelting process or melt-processed can refer to the temperature of fusion (Tm) of described resin blend or higher than this temperature of fusion under make resin blend melting to form mixture of melts and to use this mixture of melts to form the method for required product.Such as, described smelting process can comprise injection moulding, extrude, fiber sprinning and formation foam etc.
Layer separation or layering can refer to and substantially arranged by an a kind of layer of resin formation or be arranged in substantially by another layer of another kind of resin formation.Substantially the resin of type continued presence and do not form island structure in this layer in whole layer can be referred to by a kind of layer of resin formation.Described island structure can refer to that the resin portion be separated is distributed in whole resin blend.In addition, described " substantially formed " can refer to exist in one layer a kind of resin or in one layer a kind of resin exist in a large number.In layer is separated, can two-layerly to separate, or when needed, three layers or multilayer can be separated.
The present inventor finds; when use has the first resin and second resin of different physical properties; comprise the first resin with have contamination resistance the second resin for the resin blend of smelting process in can observe layer and be separated; and to extrude or during Shooting Technique or afterwards when not using extra technique; the surface of resin particle or resin uses layer to be separated and is optionally covered, thus completes the present invention.
Particularly, because described second resin has different physical propertiess, such as compared to described first resin, there is higher hydrophobicity, so such as extrude at melting process or easily can carry out layer separation in injection moulding, and described second resin can be easy to be transferred on the surface that contacts with ambient air.Therefore, when the resin blend using this for smelting process, the upper layer of resin particle or resin can not use extra coating process by described second resin formation.Therefore; by the problem be coated with or plating process causes, such as during fabrication between and increase on cost, and for the process of the coating agent that improves hardness or didirtresistance; can be resolved, obtained resin particle or the surface property of resin and contamination resistance can improve.
The layer of described resin blend is separated and can be caused by the molecular weight distribution of the physicals difference between the first resin and the second resin and/or the second resin.Herein, described different physicals, such as, can comprise surface energy, melt viscosity and solubility parameter.
In one embodiment, resin blend for smelting process comprises the first resin and the second resin, and described second resin comprises the resin that introduces the organo-functional group that fluorine or fluorine replace and is 0.1 ~ 35mN/m with the surface energy differential of described first resin at 25 ° of C.
Described first resin and described second resin can be 0.1 ~ 35mN/m at 25 ° of C surface energy differentials, preferably 1 ~ 30mN/m, and are more preferably 1 ~ 20mN/m.In described resin blend, after smelting process, the resin blend of melt-processed is exposed in ambient air.Now, this resin blend has transport property (mobility).Therefore, can hydrophobicity be had because have than the second resin of described first resin more low surface energy, and move to and contact with ambient air, so described second resin can be positioned at the position of adjacent ambient air, thus form the upper layer of resin.So when surface energy differential is very little, the layer of the resin blend of melt-processed is separated and is less likely to occur, this is because the second resin is difficult to move through the polymeric matrix of resin blend in the mixture of molten state.In addition, when surface energy differential is very large, described first resin and the second resin may not adhere to each other, thus may depart from.
In addition, the melt viscosity difference between described first resin and described second resin is at 100 ~ 1000s
-1shearing rate and described resin blend processing temperature under can be 0.1 ~ 3000pa*s, preferably 1 ~ 2000pa*s, is more preferably 1 ~ 1000pa*s.When melt viscosity difference is very little, because described first resin is easy to and described second mixed with resin, be less likely to occur so the layer of this resin blend is separated.When melt viscosity difference is very large, described first resin and the second resin may not adhere to each other, thus may depart from.
Described melt viscosity can use capillary flowmeter to measure, and is expressed as the shear viscosity (pa*s) under predetermined processing temperature and shearing rate (/s).
Described shearing rate carries out adding the shearing rate applied man-hour when described resin blend, and this shearing rate can control according to working method.
Described processing temperature is the temperature of processing described resin blend.Such as, when described resin blend such as extrude or the technique of injection moulding time, described processing temperature carries out extruding or the temperature of injection moulding.Described processing temperature can according to carrying out extruding or the resin of injection moulding controls.Such as, for the resin blend comprising the first resin be made up of ABS resin and the second resin obtained by Tri-n-butyltin methacrylate monomer polymerization, processing temperature can be 210 ~ 240 ° of C.
In addition, the solubility parameter difference between described first resin and described second resin can be 0.001 ~ 10.0 (J/cm when 25 ° of C
3)
1/2, preferably 0.01 ~ 5.0 (J/cm
3)
1/2, and be more preferably 0.01 ~ 3.0 (J/cm
3)
1/2.Solubility parameter is the intrinsic characteristic of resin, represent the solubilized ability of the polarity according to often kind of molecular resin, and the solubility parameter of often kind of resin is normally known.When solubility parameter difference is very little, because described first resin is easy to and described second mixed with resin, be less likely to occur so the layer of described resin blend is separated.When solubility parameter difference is very large, described first resin and described second resin may not adhere to each other, thus may depart from.
The molecular weight distribution (PDI) of described second resin is 1 ~ 2.5, and is preferably 1 ~ 2.3.
When the molecular weight distribution of described second resin is greater than 2.5, described first resin is easy to and this second mixed with resin due to the low molecular weight part of this second resin, or the transport property of this second resin reduces due to its high molecular weight moieties in the mixture of molten state, layer is separated and occurs hardly.
In the present invention, the weight-average molecular weight (Mw) for the second resin in the resin blend of smelting process is 30,000 ~ 200,000, and be preferably 50,000 ~ 150,000.
When described weight-average molecular weight is less than 30, when 000, described first resin is easy to and this second mixed with resin; When described weight-average molecular weight is greater than 200, when 000, the transport property of this second resin reduces, thus layer separation occurs hardly.
As mentioned above, described second resins act goes out and the difference of described first resin in physicals, and can give some functions to the surface of required resin, such as, and the surface hardness of improvement and anti-stain characteristic.
Described second resin can comprise the resin of the organo-functional group introducing fluorine or fluorine replacement.When introducing the organo-functional group of fluorine or fluorine replacement, the surface energy of this second resin or melt viscosity reduce.Thus the second resin in the mixture of molten state can be easier to mobile contact with ambient air, and such as extrude or injection moulding process in above-mentioned layer separation can more easily occur.Cause the surface energy of described second resin to reduce due to the organo-functional group replaced because of fluorine or fluorine, so the surface of described resin can have lower adhesion strength for organic or inorganic thing, thus realize excellent contamination resistance.
As the example of the organo-functional group that described fluorine replaces, can comprise: the fluorine substituted alkyl with 1 ~ 30 carbon atom; Or the fluorine with 1 ~ 30 carbon atom replaces hydroxyalkyl, and at least one or two in them can be incorporated in described resin.
More specifically, the organo-functional group that described fluorine replaces can comprise: the alkyl with 1 ~ 30 carbon atom replaced with at least three fluorine atoms, or comprises the alkyl with 1 ~ 10 carbon atom or the hydroxyalkyl of the perfluoroalkyl with 1 ~ 10 carbon atom.
The example of the organo-functional group that described fluorine replaces can comprise trifluoromethyl, trifluoroethyl, trifluoro propyl, perfluoro hexyl ethyl, five fluoropropyls, perfluoro butyl ethyl, perfluoro butyl hydroxypropyl, perfluoro hexyl hydroxypropyl, perfluoro-methyl butyl hydroxypropyl, perfluoro decyl ethyl, four fluoropropyls, octafluoro amyl group, ten difluoro heptyl and hexafluoro butyl.The example that can be included in the described resin in this second resin can comprise (methyl) acrylic resin, redix, trimethylene oxide resinoid, isocyanic ester resinoid, silicon resinoid and its multipolymer or mixture.
Described (methyl) acrylic resin makes as the acryl of main ingredient or methacryloyl monomer polymerization and the resin formed, described monomer can include but not limited to: alkyl methacrylate, such as methyl methacrylate, β-dimethyl-aminoethylmethacrylate, propyl methacrylate, butyl methacrylate, cyclohexyl methacrylate, Octyl methacrylate, lauryl methacrylate(LMA) or stearyl methacrylate; Alkyl acrylate, such as methyl acrylate, ethyl propenoate, propyl acrylate, butyl acrylate, Octyl acrylate, lauryl acrylate or stearyl acrylate alcohol ester; Or (methyl) glycidyl acrylate, such as glycidyl methacrylate or glycidyl acrylate.
Described redix is the resin comprising epoxy group(ing), can be but be not limited to: bisphenol type, such as dihydroxyphenyl propane, Bisphenol F, bisphenol S or its hydrogenation adducts (hydroadditive); Phenolic novolac type, such as phenol phenolic novolac (phenolnovolac) or cresol novolac (cresolnovolac); Nitrogenous ring-like, such as triglycidyl isocyanurate or glycolylurea; Alicyclic type; Aliphatics type; Aromatics type, such as naphthalene or biphenyl; Glycidyl type, such as glycidyl ether, glycidyl amine or glycidyl ester; Two is ring-like, such as Dicyclopentadiene (DCPD); Ester type; Or Etheric ester type.
Described trimethylene oxide resinoid be make to have at least one trimethylene oxide ring oxetane monomer polymerization and formed resin, can be but be not limited to: Isosorbide-5-Nitrae-bis-[(3-ethyl-3-oxetanylmethoxy) methyl] benzene; Two [1-ethyl (3-oxetanyl)] methyl ether; Or polyoxetane compound, such as phenol novolak resin trimethylene oxide (phenolnovolacoxetane), terephthalate dioxygen azetidine (terephthalatebisoxetane) or biphenyl dioxygen azetidine (biphenylenebisoxetane).
Described isocyanic ester resinoid is a kind of resin containing isocyanate group, can be but be not limited to: diphenylmethanediisocyanate (MDI), tolylene diisocyanate (TDI) or isophorone diisocyanate (IPDI).
Described silicon resinoid is the resin containing the main chain connected by siloxane bond (for silicon-oxygen key), can be but be not limited to polydimethylsiloxane (PDMS).
Based on described first resin of 100 weight parts, the resin blend for smelting process can comprise the second resin of 0.1 ~ 50 weight part, preferably comprises the second resin of 1 ~ 20 weight part.
Based on described first resin of 100 weight parts, when described second resin is involved with the amount being less than 0.1 weight part, layer is separated and does not occur; And when described second resin is involved with the amount being greater than 50 weight parts, manufacturing cost increases.
Described second resin can have one of thermal curable functional group and uV curable functional group, or has all thermal curable functional groups and uV curable functional group, and is not particularly limited.When thermal curable functional group is included in the second resin, hardness is caused to improve due to formed in melting process crosslinked.Therefore, described second resin is being extruded or injection moulding process can have higher surface hardness after heat cross-linking.
Meanwhile, described first resin essentially dictates the physicals of required resin, can select according to the kind of required resin and processing condition.As described first resin, synthetic resins and unrestricted can be used, but can comprise: styrene resin, such as based on the resin of acronitrile-butadiene-styrene (ABS), based on the resin of polystyrene, based on the resin of acrylonitrile styrene acrylic ester (ASA) or the resin of styrene-based-butadiene-styrene block copolymer; Polyolefin resin, such as high-density polyethylene vinyl resin, low density polyethylene vinyl resin or polyacrylics; Thermoplastic elastomer, such as ester analog thermoplastic elastomer or olefin hydrocarbons thermoplasticity elastic body; Polyoxyalkylene resinoid, such as polyoxymethylene resinoid or polyoxyethylene resinoid; Polyester resin, such as polyethylene terephthalate resinoid or polybutylene terephthalate resinoid; Polyvinyl chloride resin; Polycarbonate resin; Polyphenylene sulfide resinoid; Vinyl alcohol resin; Polyamide-based resin; Acrylic resin; Engineering plastics; Or its multipolymer or mixture.
Simultaneously, it is different that the described resin blend for smelting process can show from above-mentioned first resin in physicals, and it comprises the specific resin can giving specific function to the surface of required resin in addition, such as, wear resistant resin, anti-contamination resin, anti-fingerprint resin, pigmentary resin, nacrous resin (pearlresin), high gloss resin, matt resin, barrier resin (barrierresin) or its mixture.
The described resin blend for smelting process can adopt smelting process (such as extruding) to make resin particle.The resin particle using this resin blend to make can have following structure: wherein, first resin can be arranged at the centre of this resin particle, and the second resin can be the layer that separates with the first resin layer and is arranged to around described first resin and forms the shell of this resin particle.
According to an exemplary of the present invention, a kind of resin particle can be provided, described resin particle comprises: comprise the core of the first resin and comprise the shell of the second resin, described second resin comprises the resin of the organo-functional group introducing fluorine or fluorine replacement, and the surface energy differential of described second resin and described first resin is 0.1 ~ 35mN/m at 25 ° of C.
The molecular weight distribution of described first resin and described second resin, weight-average molecular weight and different physicalies as mentioned above, thus will be omitted its detailed description.
Meanwhile, according to another exemplary of the present invention, a kind of method preparing resin can be provided, comprise: make the described resin blend melting for smelting process to form mixture of melts; Process with to this mixture of melts.
As mentioned above; because the second resin has different physicalies; such as compared to described first resin, there is higher hydrophobicity; so extruding or can being separated by genetic horizon in injection moulding process at described resin blend; and be separated due to this layer, the surface of resin particle or resin can by optionally covering without the need to extra technique.
Particularly, described second resin can comprise the resin of the organo-functional group introducing fluorine or fluorine replacement, and the organo-functional group that this fluorine or fluorine replace can reduce surface energy or the melt viscosity of described second resin, thus such as extrude or injection moulding fusion process in there is high hydrophobicity.Therefore, described in the mixture of molten state, the second resin can be easier to mobile to contact with ambient air, and is arranged on the surface of resin due to this second resin, has the mechanical property of improvement and the resin of surface property so can provide.In addition, the organo-functional group replaced due to fluorine or fluorine can reduce the surface energy of described second resin, so the surface of described resin can have lower adhesion strength for organic or inorganic thing, and has excellent contamination resistance.
In addition, described smelting process can carry out under shear stress, and can include but not limited to injection moulding and extrude.
The described resin blend for smelting process can make resin particle by extruding.In addition, this resin blend can adopt to extrude makes resin particle, is then processed into resin by smelting process (such as injection moulding).Or described resin blend directly can make resin by injection moulding.
According in first resin extruded or use in injection moulding of described resin blend and the kind of the second resin, the temperature that will apply can be changed.
The described method preparing resin also can comprise and being cured the product obtained by described resin blend melt-processed (the melt-processed product namely obtained by described resin blend).Such as extruding or after Shooting Technique, one of thermofixation and UV-light (UV) solidification can also carried out or carry out both thermofixation and UV-light (UV) solidification.When needed, chemical treatment can be carried out after this operation.
Meanwhile, the second resin is prepared before the melt-processed that the described method preparing resin can also be included in for the resin blend of smelting process.As the example of preparation second resin, there are mass polymerization, solution polymerization, suspension polymerization or letex polymerization.
In suspension polymerization, described second resin can be obtained by following steps: by monomer dispersion in reaction medium; In reaction solvent, add the additive of such as chain-transfer agent, initiator and dispersion stabilizer and make them mix; And 40 ° of C or higher than 40 ° of C under make this polymerization of mixtures.Described monomer is the monomer of at least one resin be selected from wear resistant resin, anti-contamination resin, anti-fingerprint resin, pigmentary resin, nacrous resin, high gloss resin, matt resin, barrier resin.
The example being selected from the monomer of at least one resin in wear resistant resin, anti-contamination resin, anti-fingerprint resin, pigmentary resin, nacrous resin, high gloss resin, matt resin and barrier resin can comprise (methyl) acrylic resin, redix, trimethylene oxide resinoid, isocyanic ester resinoid, silicon resinoid or its multipolymer.
Described reaction medium can be known any medium of being generally used for preparing synthetic resins, polymkeric substance or multipolymer and unrestricted.The example of this reaction medium can be distilled water.
The described chain-transfer agent that can join in reaction solvent can be but be not limited to: alkyl sulfhydryl, such as butyl mercaptan, n-dodecyl mercaptan, tertiary lauryl mercaptan or isopropyl mercaptan; Aryl mercaptan; Halogen compounds, such as ketone tetrachloride (ketonetetrachloride); Or aromatic substance, such as α-methylstyrenedimer or α-ethyl styrene dipolymer.
Described initiator is polymerization starter, and it can be but be not limited to: superoxide, such as caprylyl peroxide, decanoyl peroxide or dodecyl superoxide; Or azo compound, such as Diisopropyl azodicarboxylate or azo two-(2,4-dimethyl) valeronitrile.
The described dispersion stabilizer that can comprise in reaction medium can be but be not limited to: organic dispersing agent, such as polyvinyl alcohol, polyolefin-maleic acid or Mierocrystalline cellulose; Or inorganic dispersant, such as tricalcium phosphate.
Described first resin and the second resin described in more detail above, thus will to omit its other description.
Meanwhile, according to another exemplary of the present invention, a kind of resin of melt-processed is provided, comprises: the first resin layer; The second resin layer that described first resin layer is formed; And the interfacial layer formed between described first resin layer and the second resin layer.Herein, described interfacial layer comprises the first resin and the second resin.In addition, described second resin layer comprises the resin of the organo-functional group introducing fluorine or fluorine replacement.The resin obtained by the resin blend comprising specific first resin and the second resin can comprise layered structure, and wherein the first resin layer is provided at its inner portion with the second resin layer in its peripheral formation.
The layer existed in the resin of melt-processed is separated and brings to the resin preparing melt-processed as described above by the application molecular weight distribution (PDI) of described second resin and the different physicals of weight-average molecular weight (Mw) and specific first resin and the second resin.The example of different physicalies can comprise surface energy, melt viscosity or solubility parameter.
Because described resin can have mechanical property and the surface property of improvement, can save for the coating or enamelling process that improve thermotolerance or resistance to marring, production time and production cost can reduce, and the productivity of the finished product can improve.
Particularly, described second resin can comprise the organo-functional group of fluorine or fluorine replacement, and due to this organo-functional group, the surface energy of described resin can reduce, thus can have low adhesion strength and excellent contamination resistance for organic or inorganic thing.
Described resin has the novel structure of this area the unknown.Described resin forms following structure: described first resin layer is separated by interfacial layer and the second resin layer, and described second resin layer is exposed in ambient air.This structure can not be formed with Shooting Technique by extruding of general resin, thus is difficult to realize the effect according to this structure.
Described first resin layer can refer to and substantially comprise the first resin and the part be arranged in described resin due to low hydrophobicity.Described second resin layer can refer to and substantially comprises the second resin and the surface hardness of surface modification of resin or the part of the anti-stain characteristic of excellence are given in the surface being arranged on described resin due to high hydrophobicity.
Meanwhile, described resin can comprise interfacial layer, and this interfacial layer comprises the blend of the first resin and the second resin, and is formed between described first resin layer and described second resin layer.Described interfacial layer can play the effect on the border formed between first resin layer and the second resin layer of layering, and comprises the blend of described first resin and the second resin.This blend can exist by this way, makes described first resin and described second resin physics or Chemical bond, and described first resin layer can pass through this blend and described second resin layers.
As mentioned above, described resin can have following structure: described first resin layer is separated by interfacial layer and described second resin layer, and described second resin layer is exposed in ambient air.Such as, described resin can have such structure: wherein said first resin layer, interfacial layer and the second resin layer order lamination; Or there is such structure: wherein, described first resin layer be set, described interfacial layer and the second resin layer be arranged at this first resin layer above and below.Or, this resin can have the first resin layer that such structure makes to be formed with multiple 3D shape (such as, spherical, circular, polyhedron and sheet) by described interfacial layer and described second resin layer order around.
Meanwhile, at sample after the cross section of low temperature impact test and this sample uses THF vapor etch, the first resin layer, the second resin layer and interfacial layer can use scanning electronic microscope (SEM) to observe.In order to observe this first resin layer and the second resin layer and interfacial layer and measure the thickness of every layer, use slicing machine device diamond tool cutting sample, thus obtain level and smooth cross section, use and compare this level and smooth cross section of solution etches that the first resin more optionally can dissolve the second resin.This cross section through etching is dissolved into the degree of depth of different levels according to the content of this first and second resin, and when this cross section is observed with miter angle from its surface by SEM, due to shade difference, this first resin layer, the second resin layer and interfacial layer can be observed, and its thickness can be measured.In the present invention, as the solution more optionally dissolving the second resin, use 1,2-dichloroethane solution (10 volume %, in EtOH), but be only an example.Therefore, can to use than any solution that there is more high resolution to described first resin described second resin and unrestricted, and this solution can change according to the kind of this second resin and composition.
The thickness of described interfacial layer can be 0.01 ~ 95% of described second resin layer and interfacial layer total thickness, and is preferably 0.1 ~ 70%.When the thickness of described interfacial layer is 0.01 ~ 95% of described second resin layer and interfacial layer total thickness, the interfacial bond strength of described first resin layer and the second resin layer is excellent.Therefore, this first resin layer and the second resin layer do not depart from, and the surface property brought by this second resin layer can be improved greatly.On the other hand, when this interfacial layer Thickness Ratio described in the second resin layer and interfacial layer total thickness much smaller time, bond strength between this first resin layer and second resin layer reduces, thus two-layerly may depart from.But when the thickness of this interfacial layer is very thick, the improvement of the surface property of this second resin layer may not be remarkable.
The thickness of described second resin layer can be 0.01 ~ 60% of this resin total thickness, is preferably 0.1 ~ 40%, and is more preferably 1 ~ 20%.Because this second resin layer has the thickness in pre-determined range, so predetermined function can be provided to the surface of this resin.Herein, when this second resin layer has very thin thickness, the surface property substantially improving this resin may be difficult to; When this second resin layer has very thick thickness, the mechanical property of this second resin may embody in this resin, thus the mechanical property of this first resin may change.
The organo-functional group of described first resin and the second resin and fluorine replacement describes in detail above, thus will omit its other description.
Meanwhile, according to another exemplary of the present invention, a kind of resin of melt-processed of the second resin layer comprising the first resin layer and formed on described first resin layer can be provided.Herein, the composition of this first resin layer is detected from the surface of this second resin layer by infrared (IR) spectrograph, and this second resin layer comprises the resin of the organo-functional group introducing fluorine or fluorine replacement.
The structure of this resin, that is, the wherein structure that gone out from the Surface testing of this second resin layer by IR spectrograph of the composition of this first resin layer, be novel, and not yet know in the art.Generally speaking, in coating process, the composition of the first resin layer be difficult to from the Surface testing of this second resin layer to.
The surface of described second resin layer refers to and is exposed to ambient air and the surface not being exposed to the first resin layer.
In addition, the composition of described first resin layer refers at least one composition comprised in this first resin layer.
Described first resin and the second resin and to introduce the resin of the organo-functional group that fluorine replaces described in more detail above, thus its other description will be omitted.
According to another exemplary of the present invention, the trolley part of the resin comprising described melt-processed, the helmet, electrical device components, spinning machine parts, toy or pipe can be provided.
Beneficial aspects
According to the present invention, the resin blend of smelting process, resin particle can be provided for, use them to prepare method and the resin of resin.This resin blend can improve the mechanical property of resin and surface property and achieve excellent contamination resistance.In addition, do not need extra coating owing to manufacturing resin, so manufacturing time and/or manufacturing cost can reduce, and productivity can improve.
Accompanying drawing explanation
Fig. 1 is the SEM image of the cross-sectional view illustrated according to the obtained hierarchical tree grease article of embodiment 2.
Fig. 2 is when observing from surface with miter angle, illustrates with can the SEM image of the cross-sectional view of resin crossed of the solution-treated of selective dissolution second resin.
Embodiment
The present invention is described in detail with reference to the following examples.But the present invention is not limited to the following examples.
EXPERIMENTAL EXAMPLESThe 1: the measurement of surface energy
According to Owens-Wendt-Rabel-Kaelble (OWRK) method, the surface energy of the first resin obtained by embodiment and comparative example and the second resin uses Drop Shape Analyzer (Kruss, DSA100) to measure.
More specifically, by the first resin or the second resin dissolves in methyl acetate to have the concentration of 15wt%, then use stick coating method to be coated on LCD glass.The LCD glass of this coating in the baking oven of 60 ° of C predrying 2 minutes, then in the baking oven of 90 ° of C dry 1 minute.
After dry (or solidification), deionized water and methylene iodide to be dropped in respectively on the surface of coating 10 times at 25 ° of C, thus to obtain the mean value of contact angle, surface energy calculates by being updated in OWRK method by numerical value.
EXPERIMENTAL EXAMPLESThe 2: the measurement of melt viscosity
The melt viscosity of the first resin obtained by embodiment and comparative example and the second resin uses capillary rheometer 1501 (Gottfert) to measure.
More specifically, kapillary die head is being connected to after in cylinder, this first resin or the second resin is being divided into 3 parts and puts in cylinder.Measure according to 100 ~ 1000s under the processing temperature of 240 ° of C
-1the shear viscosity (pa*s) of shearing rate.
EXPERIMENTAL EXAMPLESThe 3: the measurement of solubility parameter
Although there is the method for some measurements and calculations solubility parameters, but in embodiment below and comparative example, use known method, VanKrevelen method is [with reference to Bicerano, J., PredictionofPolymerProperties, the third edition, MarcelDekkerInc., NewYork (2002), the disclosure content is all included in this specification sheets by reference], calculate solubility parameter at 25 ° of C.According to VanKrevelen method, solubility parameter uses group contribution theory (groupcontributiontheory) to calculate, and is defined as formula below:
In above-mentioned formula, E
cohbe internal cohesive energy, V is molecular volume and e
cohit is cohesive energy density(CED).This internal cohesive energy (E
coh) be defined as follows:
E
coh＝10570.9×(
0χ
v-
0χ)+9072.8×(2×
1χ-
1χ
v)+1018.2×N
VKH
In formula above,
0x,
1x,
0x
vwith
1x
vconnectivity Index of Electronic Density, and N
vKHit is associations.Each variable is calculated with reference to disclosed document [Bicerano, J., PredictionofPolymerProperties, the third edition, MarcelDekkerInc., NewYork (2002)].
EXPERIMENTAL EXAMPLESThe 4: the observation of cross section characteristic
Sample obtained in embodiment and comparative example is through low temperature impact test.Then, the fracture surface of this sample uses THF steam to etch, and uses SEM to observe the cross section of layering.
Simultaneously, in order to the thickness of the first resin layer and the second resin layer and interfacial layer of measuring layering, the sample of embodiment and comparative example uses slicing machine device (LeicaEMFC6) to cut under-120 ° of C with diamond tool below, thus obtains level and smooth cross section.The sample part of the level and smooth cross section with section is immersed in (10 volume %, in EtOH) in 1,2-dichloroethane solution and, to etch 10 minutes, then uses distilled water wash.Cross-section parts through etching is dissolved into the degree of depth of different levels according to the content of this first and second resin, and SEM can be used to observe.That is, when this cross section is observed with miter angle from its surface, due to shade difference, this first resin layer, the second resin layer and interfacial layer can be observed, and the thickness of each layer can be measured.The feature of this cross section observed with miter angle from its surface is shown in Figure 2.
EXPERIMENTAL EXAMPLESThe 5: the experiment of measuring pencil hardness
The pencil hardness of the sample of embodiment and comparative example uses pencil hardness tester (ChungbukTech) to measure under the firm demand of 500g.With 45 degree of fixed angles standard pencil (Mitsubishi; 6B to 9H level) mark cut on the surface of the samples, observe the velocity of variation (ASTM3363) on surface thus.Pencil Hardness values is the mean value of the result drawn by the test carrying out 5 times.
EXPERIMENTAL EXAMPLESThe 6: the measurement of molecular weight distribution (PDI)
Gel permeation chromatography (GPC) is used to measure molecular weight distribution under the following conditions:
Instrument: 1200 series of being produced by AgilentTechnologies
Chromatographic column: the 2PLgelmixedBs produced by PolymerLaboratories
Solvent: THF
Column temperature: 40 ° of C
Sample concentration: 1mg/mL, 100L sample introduction (injection)
Standard: polystyrene (Mp:3900000,723000,316500,52200,31400,7200,3940 or 485)
As routine analyzer, the ChemStataion provided by AgilentTechnologies is provided, weight-average molecular weight (Mw) and number-average molecular weight (Mn) use gel permeation chromatography (GPC) to measure, and then molecular weight distribution is calculated by equation Mw/Mn.
EXPERIMENTAL EXAMPLESThe 7: the test of measuring contamination resistance
Measure the contamination resistance of the sample obtained in embodiment and comparative example.Specifically, by this sample dissolution in methyl acetate to 15wt%, and adopt stick coating method to be coated on LCD glass.Subsequently, by the LCD glass of this coating in 60 ° of C baking ovens predrying 2 minutes, and in the baking oven of 90 ° of C dry 1 minute.
Then, after writing on the sample surfaces of drying with pen (pen name, Monami), draw two lines that about 5cm is long, and wipe with the supatex fabric of ultra-fine fibre the vestige stayed with the pen that detects by an unaided eye.When the vestige of pen is removed completely, repeats and continue above-mentioned steps until the vestige of pen can not be removed.The total degree of record repeating step.
EXPERIMENTAL EXAMPLESThe 8: use IR spectrograph to carry out surface analysis
Use is equipped with VarianFTS-7000 spectrograph (Varian, USA) and the UMA-600IR microscope of mercury cadmium tellurium (MCT) detector test, the detection of spectrum and data processing use Win-IRPRO3.4 software (Varian, USA) to carry out.Experiment condition is as follows:
-specific refractory power is germanium (Ge) atr crystal of 4.0
-mid-infrared spectral the spectral resolution that obtained by attenuated total reflectance attenuated total refraction: 8cm
-1with the scope of 16 scannings: 4000cm
-1-600cm
-1.
Internal reference wave band (InternalReferenceBand): carbonyl (the C=Ostr., ~ 1725cm of acrylate
-1)
The initial component of the first resin: adiene cpd [C=Cstr. (~ 1630cm
-1) or=C-H out-of-plane vibration (out-of-planevib.) (~ 970cm
-1)]
Calculate peak intensity ratio [I
bD(C=C)/I
a] and [I (C=O)
bD(out-of-plane)/I
a(C=O)], the detection of spectrum carries out 5 times in the different zones of a sample, and calculating mean value and standard deviation.
embodiment 1
The preparation of (1) second resin
Using 1500g distilled water and 4g as dispersion agent 2% polyvinyl alcohol water solution put into the reactor of 3 liters and make it dissolve.Then, in addition using 760g methyl methacrylate, 40g methacrylic acid perfluoro hexyl ethyl ester, 2.4g as the n-dodecyl mercaptan of chain-transfer agent and 2.4g as the azo two-(2 of initiator, 4-dimethyl) valeronitrile adds wherein, and mixing is stirred with 400rpm simultaneously.This mixture is carried out 3 hours polyreactions under 60 ° of C, is cooled to 30 ° of C, thus obtain pearl second resin.Afterwards, by this second resin distilled water wash three times, dehydration is also dry in an oven.
(2) preparation of the resin of resin blend and this resin blend of use
After by the second resin alloy of the first resin of 90 weight parts (thermoplastic resin be made up of the vinylbenzene of the methyl methacrylate of 60wt%, the vinyl cyanide of 7wt%, the divinyl of 10wt% and 23wt%) and 10 weight parts, use twin screw extruder (Leistritz) to extrude this blend under 240 ° of C, thus obtain resin particle.Then, under 240 ° of C, use EC100 Ф 30 injection moulding machine (ENGEL) to carry out injection moulding to above-mentioned resin particle, thus obtain the sample 1 that thickness is 3200 μm.
(3) measurement of sample physicals
As the measuring result of the physicals of obtained sample, the thickness demonstrating the second resin layer is 102 μm, and the thickness of interfacial layer is 15 μm, and the difference in surface energy is 5.4mN/m, difference in melt viscosity is 250pa*s, and the difference in solubility parameter is 0.2 (J/cm
3)
1/2, the weight-average molecular weight of this second resin obtained by GPC is 100K, and its molecular weight distribution is 2.In addition, contact angle is 75 degree, and pencil hardness is 2H, there is layer and is separated.In the evaluation of contamination resistance, carry out testing until the number of times repeated when vestige is no longer removed is 40.
Peak intensity ratio [the I recorded by IR spectrograph
bD(C=C)/I
a(C=O)] have the mean value of 0.0113, standard deviation is 0.0002 simultaneously; Peak intensity ratio [I
bD(out-of-plane)/I
a(C=O)] have the mean value of 0.398, standard deviation is 0.0021 simultaneously.
embodiment 2
The preparation of (1) second resin
Except using 552g methyl methacrylate, 240g3-ethyl-3-methacryloxymethyl trimethylene oxide and 8g methacrylic acid perfluoro hexyl ethyl substituted 760g methyl methacrylate and 40g methacrylic acid perfluoro hexyl ethyl ester, utilize and obtain the second resin with the same procedure that describes in embodiment 1.
(2) preparation of the moulded product of resin blend and this resin blend of use
By the first resin alloy of the second resin obtained above for 10 weight parts and 90 weight parts, then to prepare with the same procedure that describes in embodiment 1 sample that thickness is 3200 μm.
(3) measurement of sample physicals
As the measuring result of the physicals of obtained sample, the thickness demonstrating the second resin layer is 14 μm, and the thickness of interfacial layer is 13 μm, and the difference in surface energy is 11.9mN/m, difference in melt viscosity is 280pa*s, and the difference in solubility parameter is 0.5 (J/cm
3)
1/2, the weight-average molecular weight of this second resin obtained by GPC is 100K, and its molecular weight distribution is 2.1.In addition, contact angle is 82 degree, and pencil hardness is 2H, and there is layer separation.In the evaluation of contamination resistance, carry out testing until the number of times repeated when vestige is no longer removed is 21.
embodiment 3
The preparation of (1) second resin
Except using 760g methyl methacrylate and 40g methacrylic acid perfluor ester in the last of the ten Heavenly stems to replace except 760g methyl methacrylate and 40g methacrylic acid perfluoro hexyl ethyl ester, obtained second resin of same procedure adopting and describe in embodiment 1.
(2) preparation of the moulded product of resin blend and this resin blend of use
By the first resin alloy of above-mentioned the second obtained resin of 10 weight part and 90 weight parts, then to prepare with the same procedure that describes in embodiment 1 sample that thickness is 3200 μm.
(3) measurement of sample physicals
As the measuring result of the physicals of obtained sample, the thickness demonstrating the second resin layer is 50 μm, and the thickness of interfacial layer is 21 μm, and the difference in surface energy is 7.3mN/m, difference in melt viscosity is 260pa*s, and the difference in solubility parameter is 0.2 (J/cm
3)
1/2, the weight-average molecular weight of this second resin obtained by GPC is 100K, and its molecular weight distribution is 2.In addition, contact angle is 83 degree, and pencil hardness is 1.5H, and there is layer separation.In the evaluation of contamination resistance, carry out testing until the number of times repeated when vestige is no longer removed is 15.
embodiment 4
The preparation of (1) second resin
Except use 680g methyl methacrylate and 120g methacrylic acid perfluoro hexyl ethyl substituted 760g methyl methacrylate and 40g methacrylic acid perfluoro hexyl ethyl ester, obtained second resin of same procedure adopting and describe in embodiment 1.
(2) preparation of the moulded product of resin blend and this resin blend of use
By the first resin alloy of above-mentioned the second obtained resin of 10 weight part and 90 weight parts, then to obtain with the same procedure that describes in embodiment 1 sample that thickness is 3200 μm.
(3) measurement of sample physicals
As the measuring result of the physicals of obtained sample, the thickness demonstrating the second resin layer is 120 μm, and the thickness of interfacial layer is 40 μm, and the difference in surface energy is 14.5mN/m, difference in melt viscosity is 310pa*s, and the difference in solubility parameter is 0.5 (J/cm
3)
1/2, the weight-average molecular weight of this second resin obtained by GPC is 100K, and its molecular weight distribution is 2.1.In addition, contact angle is 86 degree, and pencil hardness is 2.5H, and there is layer separation.In the evaluation of contamination resistance, carry out testing until the number of times repeated when vestige is no longer removed is 50.
embodiment 5
The preparation of (1) second resin
Except using 520g methyl methacrylate, 240g3-ethyl-3-methacryloxymethyl trimethylene oxide and 40g methacrylic acid perfluoro hexyl ethyl substituted 760g methyl methacrylate and 40g methacrylic acid perfluoro hexyl ethyl ester, obtained second resin of same procedure adopting and describe in embodiment 1.
(2) preparation of the moulded product of resin blend and this resin blend of use
By the first resin alloy of above-mentioned the second obtained resin of 10 weight part and 90 weight parts, then to obtain with the same procedure that describes in embodiment 1 sample that thickness is 3200 μm.
(3) measurement of sample physicals
As the measuring result of the physicals of obtained sample, the thickness demonstrating the second resin layer is 125 μm, and the thickness of interfacial layer is 10 μm, and the difference in surface energy is 15.1mN/m, difference in melt viscosity is 290pa*s, and the difference in solubility parameter is 0.6 (J/cm
3)
1/2, the weight-average molecular weight of this second resin obtained by GPC is 100K, and its molecular weight distribution is 2.1.In addition, contact angle is 88 degree, and pencil hardness is 2H, and there is layer separation.In the evaluation of contamination resistance, carry out testing until the number of times repeated when vestige is no longer removed is 62.
embodiment 6
The preparation of (1) second resin
Except using 560g methyl methacrylate, 200g cyclohexyl methacrylate and 40g methacrylic acid perfluoro hexyl ethyl substituted 760g methyl methacrylate and 40g methacrylic acid perfluoro hexyl ethyl ester, obtained second resin of same procedure adopting and describe in embodiment 1.
(2) preparation of the moulded product of resin blend and this resin blend of use
By the first resin alloy of above-mentioned the second obtained resin of 10 weight part and 90 weight parts, then to obtain with the same procedure that describes in embodiment 1 sample that thickness is 3200 μm.
(3) measurement of sample physicals
As the measuring result of the physicals of obtained sample, the thickness demonstrating the second resin layer is 10 μm, and the thickness of interfacial layer is 22 μm, and the difference in surface energy is 7.4mN/m, difference in melt viscosity is 410pa*s, and the difference in solubility parameter is 0.6 (J/cm
3)
1/2, the weight-average molecular weight of this second resin obtained by GPC is 100K, and its molecular weight distribution is 2.In addition, contact angle is 84 degree, and pencil hardness is 2H, and there is layer separation.In the evaluation of contamination resistance, carry out testing until the number of times repeated when vestige is no longer removed is 30.
embodiment 7
The preparation of (1) second resin
Except using 380g methyl methacrylate, 380g cyclohexyl methacrylate and 40g methacrylic acid perfluoro hexyl ethyl substituted 760g methyl methacrylate and 40g methacrylic acid perfluoro hexyl ethyl ester, obtained second resin of same procedure adopting and describe in embodiment 1.
(2) preparation of the moulded product of resin blend and this resin blend of use
By the first resin alloy of above-mentioned the second obtained resin of 10 weight part and 90 weight parts, then to obtain with the same procedure that describes in embodiment 1 sample that thickness is 3200 μm.
(3) measurement of sample physicals
As the measuring result of the physicals of obtained sample, the thickness demonstrating the second resin layer is 45 μm, and the thickness of interfacial layer is 10 μm, and the difference in surface energy is 5.5mN/m, difference in melt viscosity is 450pa*s, and the difference in solubility parameter is 0.8 (J/cm
3)
1/2, the weight-average molecular weight of this second resin obtained by GPC is 100K, and its molecular weight distribution is 2.In addition, contact angle is 83 degree, and pencil hardness is 2.5H, and there is layer separation.In the evaluation of contamination resistance, carry out testing until the number of times repeated when vestige is no longer removed is 35.
comparative example 1
The preparation of (1) second resin
Except using 560g methyl methacrylate and 240g3-ethyl-3-methacryloxymethyl trimethylene oxide to replace except 760g methyl methacrylate and 40g methacrylic acid perfluoro hexyl ethyl ester, obtained second resin of same procedure adopting and describe in embodiment 1.
(2) preparation of the moulded product of resin blend and this resin blend of use
By the first resin alloy of above-mentioned the second obtained resin of 10 weight part and 90 weight parts, then to prepare sample with the same procedure that describes in embodiment 1.
(3) measurement of sample physicals
As the measuring result of the physicals of obtained sample, the thickness demonstrating the second resin layer is 80 μm, and the thickness of interfacial layer is 30 μm, and the difference in surface energy is 1mN/m, difference in melt viscosity is 280pa*s, and the difference in solubility parameter is 0.5 (J/cm
3)
1/2, the weight-average molecular weight of this second resin obtained by GPC is 100K, and its molecular weight distribution is 2.In addition, contact angle is 68 degree, and pencil hardness is 2H, and there is layer separation.In the evaluation of contamination resistance, in first time test, vestige is not completely removed.
comparative example 2
The preparation of (1) second resin
Except using 560g methyl methacrylate and 240g methacrylic acid 3-cyclohexyl to replace except 760g methyl methacrylate and 40g methacrylic acid perfluoro hexyl ethyl ester, obtained second resin of same procedure adopting and describe in embodiment 1.
(2) preparation of the moulded product of resin blend and this resin blend of use
By the first resin alloy of above-mentioned the second obtained resin of 10 weight part and 90 weight parts, then to prepare sample with the same procedure that describes in embodiment 1.
(3) measurement of sample physicals
As the measuring result of the physicals of obtained sample, the thickness demonstrating the second resin layer is 76 μm, and the thickness of interfacial layer is 23 μm, and the difference in surface energy is 1.4mN/m, difference in melt viscosity is 410pa*s, and the difference in solubility parameter is 0.6 (J/cm
3)
1/2, the weight-average molecular weight of this second resin obtained by GPC is 100K, and its molecular weight distribution is 1.9.In addition, contact angle is 74 degree, and pencil hardness is 2H, and there is layer separation.In the evaluation of contamination resistance, in first time test, vestige does not remove completely.
comparative example 3
By dry in an oven for the resin particle of the first resin of 100 weight parts, and use EC100 Ф 30 injection moulding machine (ENGEL) to carry out injection moulding at 240 ° of C, thus obtain sample.
As the measuring result of the physicals of obtained sample, surface energy is 43mN/m, and contact angle is 69 degree, and pencil hardness is F.In the evaluation of contamination resistance, in first time test, vestige is not completely removed.
comparative example 4
The preparation of (1) second resin
Except using 1.6g as the n-dodecyl mercaptan of chain-transfer agent and the 0.9g azo two-(2 as initiator, 4-dimethyl) valeronitrile replaces 2.4g n-dodecyl mercaptan and 2.4g azo two-(2,4-dimethyl) outside valeronitrile, adopt and prepare the second resin with the same procedure that describes in embodiment 1.
(2) preparation of the moulded product of resin blend and this resin blend of use
By the first resin alloy of above-mentioned the second obtained resin of 10 weight part and 90 weight parts, then to prepare sample with the same procedure that describes in embodiment 1.
(3) measurement of sample physicals
As the measuring result of the physicals of obtained sample, the difference demonstrated in surface energy is 4mN/m, and the difference in melt viscosity is 400pa*s, and the difference in solubility parameter is 0.5 (J/cm
3)
1/2, the weight-average molecular weight of this second resin obtained by GPC is 100K, and its molecular weight distribution is 3.2.In addition, contact angle is 72 degree, and pencil hardness is 0.5H, and there is not layer separation.In the evaluation of contamination resistance, carry out testing until the number of times repeated when vestige is no longer removed is 3.
comparative example 5
By using Mayerbar#9 to be coated with anti-contamination and to be firmly coated with feed liquid (comprising multifunctional polyacrylic ester), 60 ~ 90 ° of C these coatings dry 4 minutes to form film, and working strength is 3000mJ/cm
2this film of ultraviolet radiation-curable, carry out form layers, thus hard coat is formed on the sample of comparative example 3, described anti-contamination is firmly coated with feed liquid (17.5wt%DPHA, 10wt%PETA, 1.5wt% methacrylic acid perfluoro hexyl ethyl ester, 5wt% from urethane acrylate EB1290,45wt% methyl ethyl ketone of SKcytech, 20wt% Virahol and 1wt% from the IRGACURE184 of Ciba as ultraviolet initiator) and is obtained by the present inventor.
The pencil hardness of above-mentioned hard coat is 3H, in the evaluation of contamination resistance, carries out testing until the number of times repeated when pen vestige is no longer removed is 50.In addition, the peak intensity ratio [I detected by IR spectrograph
bD(C=C)/I
a] and [I (C=O)
bD(out-of-plane)/I
a(C=O) mean value] and standard deviation are 0 respectively.
Claims (14)
1., for a resin blend for smelting process, comprising:
First resin; With
Second resin, this second resin comprises the resin of the organo-functional group introducing fluorine or fluorine replacement, and the surface energy differential of this second resin and described first resin is 0.1 ~ 35mN/m at 25 DEG C,
The organo-functional group that described fluorine replaces comprises at least one in the fluorine substituted alkyl being selected from and having 1 ~ 30 carbon atom and the replacement of the fluorine with 1 ~ 30 carbon atom hydroxyalkyl,
Wherein, the molecular weight distribution of described second resin is 1 ~ 2.3, and weight-average molecular weight is 30,000 ~ 200,000,
Described blend carries out can forming layered structure in melt-processed process under shear stress.
2. resin blend according to claim 1, wherein, the surface energy differential between described first resin and described second resin is 0.1 ~ 30mN/m at 25 DEG C.
3. resin blend according to claim 1, wherein, the melt viscosity difference between described first resin and described second resin is at 100 ~ 1000s
-1shearing rate and described resin blend processing temperature under be 0.1 ~ 3000pas.
4. resin blend according to claim 1, wherein, the solubility parameter difference between described first resin and described second resin is 0.001 ~ 10.0 (J/cm at 25 DEG C
3)
1/2.
5. resin blend according to claim 1, wherein, the resin introducing the organo-functional group that fluorine or fluorine replace described in comprise be selected from (methyl) acrylic resin, redix, at least one in trimethylene oxide resinoid, isocyanic ester resinoid, silicon resinoid and multipolymer thereof.
6. resin blend according to claim 1, wherein, described first resin comprises at least one be selected from styrene resin, polyolefin resin, thermoplastic elastomer, polyoxyalkylene resinoid, polyester resin, polyvinyl chloride resin, polycarbonate resin, polyphenylene sulfide resinoid, vinyl alcohol resin, acrylic resin and multipolymer thereof.
7. a resin particle, comprising:
Comprise the core of the first resin; With
Comprise the shell of the second resin, described second resin comprises the resin of the organo-functional group introducing fluorine or fluorine replacement, and the surface energy differential of described second resin and described first resin is 0.1 ~ 35mN/m at 25 DEG C,
The organo-functional group that described fluorine replaces comprises at least one in the fluorine substituted alkyl being selected from and having 1 ~ 30 carbon atom and the replacement of the fluorine with 1 ~ 30 carbon atom hydroxyalkyl,
Wherein, the molecular weight distribution of described second resin is 1 ~ 2.3, and weight-average molecular weight is 30,000 ~ 200,000,
Described resin particle has the layered structure carrying out under shear stress being formed in melt-processed process.
8. prepare a method for resin, comprising:
Make resin blend melting according to claim 1, thus form mixture of melts; With
This mixture of melts is processed.
9. method according to claim 8, the melt-processed product also comprised being obtained by described resin blend is cured.
10. method according to claim 8, wherein, described melting and processing are carried out under shear stress.
11. methods according to claim 9, wherein, described solidification utilizes thermofixation or ultraviolet light polymerization to carry out.
12. 1 kinds of methods preparing resin, comprising:
Make resin particle melting according to claim 7, thus form melt; With
Described melt is processed.
The resin of 13. 1 kinds of melt-processed, comprising:
First resin layer, this first resin layer comprises the first resin;
The second resin layer that described first resin layer is formed, this second resin layer comprises the second resin, and the surface energy differential of this second resin and described first resin is 0.1 ~ 35mN/m at 25 DEG C; With
Comprise the first resin and the second resin and the interfacial layer formed between described first resin layer and the second resin layer,
Wherein, described second resin comprises the resin of the organo-functional group introducing fluorine or fluorine replacement, and the organo-functional group that described fluorine replaces comprises at least one in the fluorine substituted alkyl being selected from and having 1 ~ 30 carbon atom and the replacement of the fluorine with 1 ~ 30 carbon atom hydroxyalkyl
Wherein, the molecular weight distribution of described second resin is 1 ~ 2.3, and weight-average molecular weight is 30,000 ~ 200,000,
Described resin has the layered structure carrying out under shear stress being formed in melt-processed process.
14. resins according to claim 13, wherein, adopt infrared spectrometer on the surface of described second resin layer, detect the composition of described first resin layer.
Applications Claiming Priority (9)
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| KR10-2010-0050639 | 2010-05-28 | ||
| KR20100050639 | 2010-05-28 | ||
| KR10-2010-0100385 | 2010-10-14 | ||
| KR20100100385 | 2010-10-14 | ||
| KR1020110050289A KR101560022B1 (en) | 2010-05-28 | 2011-05-26 | Resin blend for melting process, pellet and preparation method of resin molded article using the same, and resin molded article |
| KR10-2011-0050298 | 2011-05-26 | ||
| KR10-2011-0050289 | 2011-05-26 | ||
| KR1020110050298A KR101604878B1 (en) | 2010-05-28 | 2011-05-26 | Melt processed resin molded article |
| PCT/KR2011/003882 WO2011149294A2 (en) | 2010-05-28 | 2011-05-26 | Resin blend for melt-processing, pellet, method for manufacturing resin-molded product using same and resin-molded product |
Publications (2)
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| CN102918112A CN102918112A (en) | 2013-02-06 |
| CN102918112B true CN102918112B (en) | 2016-01-13 |
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| US (1) | US9090763B2 (en) |
| EP (1) | EP2578639B1 (en) |
| KR (2) | KR101604878B1 (en) |
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| CN104066799B (en) * | 2011-11-25 | 2016-06-01 | Lg化学株式会社 | Resin blend |
| EP2801590A4 (en) * | 2011-11-25 | 2015-10-28 | Lg Chemical Ltd | Resin mixture |
| KR101640630B1 (en) * | 2011-11-25 | 2016-07-18 | 주식회사 엘지화학 | Resin blend |
| TWI478813B (en) * | 2012-12-25 | 2015-04-01 | Chi Mei Corp | Resin laminate |
| CN103674886A (en) * | 2013-12-05 | 2014-03-26 | 广州市纤维产品检测院 | Determination method for components in inner and external layers of skin-core-structured dual-component high polymer fiber |
| US10472513B2 (en) * | 2015-06-30 | 2019-11-12 | Dow Global Technologies Llc | Polymeric formulation with dirt pick-up resistance |
| CN107924912B (en) * | 2016-03-31 | 2020-09-11 | 株式会社Lg化学 | Semiconductor device and method for manufacturing the same |
| CN106976290B (en) * | 2017-03-15 | 2019-01-04 | 嘉浦薄膜新材料（昆山）有限公司 | High-performance is packed for laminated film |
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| NL7713407A (en) * | 1976-12-16 | 1978-06-20 | Rohm & Haas | PROCESS FOR PREPARING MOLDING MIXTURES BASED ON ACRYLIC POLYMER. |
| US5855977A (en) | 1996-08-26 | 1999-01-05 | Minnesota Mining And Manufacturing Company | Multi-layer compositions comprising a fluoropolymer |
| JP2000239532A (en) * | 1999-02-19 | 2000-09-05 | Sekisui Chem Co Ltd | Thermoplastic resin composition |
| US6818173B1 (en) * | 2000-08-10 | 2004-11-16 | Northwestern University | Polymeric blends formed by solid state shear pulverization and having improved melt flow properties |
| US6849314B2 (en) * | 2002-04-18 | 2005-02-01 | 3M Innovative Properties Company | Fluoropolymer blends and multilayer articles |
| JP2004307707A (en) | 2003-04-09 | 2004-11-04 | Teijin Chem Ltd | Method for producing resin composition and resin pellet produced by the production method |
| JP4907898B2 (en) * | 2005-04-26 | 2012-04-04 | 旭化成ケミカルズ株式会社 | Thermoplastic resin molding |
| JP5103611B2 (en) * | 2006-06-12 | 2012-12-19 | 国立大学法人北海道大学 | Multiphase polymer fine particles and production method thereof |
| MX2009001339A (en) * | 2006-08-04 | 2009-02-16 | Arkema France | Photovoltaic modules having a polyvinylidene fluoride surface. |
| KR100796940B1 (en) | 2006-11-07 | 2008-01-22 | (주)고려소재연구소 | Hard-coating composition using for polycarbonate panel |
| KR101148803B1 (en) * | 2007-08-24 | 2012-05-24 | 토탈 페트로케미칼스 리서치 펠루이 | Polyethylene and polyhydroxy carboxylic acid blends |
| KR100876260B1 (en) | 2007-10-19 | 2008-12-26 | 금호석유화학 주식회사 | High transparence and high heat resistance thermoplastic risin composition and a manufacturing method thereof |
| KR101373436B1 (en) * | 2010-05-28 | 2014-03-13 | 주식회사 엘지화학 | Resin blend for melting process, pellet and preparation method of resin molded article using the same |
| KR101640630B1 (en) * | 2011-11-25 | 2016-07-18 | 주식회사 엘지화학 | Resin blend |
| EP2801590A4 (en) * | 2011-11-25 | 2015-10-28 | Lg Chemical Ltd | Resin mixture |
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- 2011-05-26 KR KR1020110050298A patent/KR101604878B1/en not_active Application Discontinuation
- 2011-05-26 KR KR1020110050289A patent/KR101560022B1/en active IP Right Grant
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- 2011-05-26 WO PCT/KR2011/003882 patent/WO2011149294A2/en active Application Filing
- 2011-05-26 CN CN201180026466.3A patent/CN102918112B/en active Active
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| Publication number | Publication date |
|---|---|
| KR20110131126A (en) | 2011-12-06 |
| WO2011149294A3 (en) | 2012-05-03 |
| WO2011149294A2 (en) | 2011-12-01 |
| KR101560022B1 (en) | 2015-10-15 |
| EP2578639A4 (en) | 2014-05-28 |
| US9090763B2 (en) | 2015-07-28 |
| CN102918112A (en) | 2013-02-06 |
| US20130164535A1 (en) | 2013-06-27 |
| EP2578639B1 (en) | 2019-08-07 |
| EP2578639A2 (en) | 2013-04-10 |
| KR101604878B1 (en) | 2016-03-18 |
| KR20110131127A (en) | 2011-12-06 |
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